Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → (R)-2-(4-cyano-2-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-3-phenylpropanamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Binap, (A+-)- | HCID 634876 | — |
| 반응물 | 3-Methylisothiazol-5-ylamine hydrochloride | HCID 2723918 | — |
| 반응물 | (R)-2-(5-bromo-4-cyano-2-fluorophenylamino)-3-phenylpropanamide | HCID 67508222 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (R)-2-(4-cyano-2-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-3-phenylpropanamide | HCID 67508807 | — |
반응 단계
A mixture of (R)-2-(5-bromo-4-cyano-2-fluorophenylamino)-3-phenylpropanamide (362 mg, 1.00 mmol), 5-amino-3-methylisothiazole hydrochloride (166 mg, 1.10 mmol), BINAP (70 mg, 0.112 mmol), Pd(OAc)2 (35 mg, 0.156 mmol) and K2CO3 (430 mg, 3.11 mmol) in dioxane (5 mL) was degassed with Ar, then was stirred at 120 C for 18 h. More Pd(OAc)2 (35 mg, 0.156 mmol) was added. The mixture was stirred at 120 C for another 18 h. Water and EtOAc were added. After being filtered, the filtrate was washed with water, dried over Na2SO4, concentrated in vacuo to give (R)-2-(4-cyano-2-fluoro-5-(3-methylisothiazol-5-ylamino)phenylamino)-3-phenylpropanamide as a crude residue.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08846928B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-8864d7801c66454185a1b0b630c6c300 |
| 출처 메모 | uspto-grants-2014_09 |